Potassium Carbonate → 2,9-Diazatricyclo[5.3.0.0,2,5]decane

HRID 1646004Notes

Reaction equation

HRID 1646004 reaction equation
[N:1]12[CH2:10][CH2:9][CH:8]1[CH2:7][CH:6]1[CH:2]2[CH2:3][N:4](C(OCC)=O)[CH2:5]1.C(=O)([O-])[O-].[K+].[K+]>O>[N:1]12[CH2:10][CH2:9][CH:8]1[CH2:7][CH:6]1[CH:2]2[CH2:3][NH:4][CH2:5]1

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 54190177Ethyl 1,4-diazatricyclo [6.2.0.02,6]decane-4-carboxylate

Product 1

HCID 162289032,9-Diazatricyclo[5.3.0.0,2,5]decane

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

13.7 g (65.1 mmol) of ethyl 1,4-diazatricyclo[6.2.0.02,6 ]decane-4-carboxylate are heated under reflux overnight with 42 g of Ba(OH)2.8H2O in 150 ml of water. Potassium carbonate is added, barium carbonate is filtered off with suction and the filtrate is extracted ten times using 100 ml of chloroform each time. The extracts are dried over potassium carbonate and concentrated, and the residue is distilled.

Workup

  1. filtrationbarium carbonate is filtered off with suction
  2. extractionthe filtrate is extracted ten times
  3. dry with materialThe extracts are dried over potassium carbonate
  4. concentrationconcentrated
  5. distillationthe residue is distilled

Sources & evidence

ORD record
ord-3f63fa43df484b03a459c9099c6523cc
Source dataset
uspto-grants-1993_01
Patent number
US05177210

Reaction notes

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